Hydrochloric Acid → HCID 19705663, Verbindung

A ethanol (5 mL) solution of nitrocyclohexane (5.00 g, 38.7 mmol) and sodium hydroxide (12.5 g, 0.3 mmol) was heated to 55° C., 35% formalin solution (3.0 mL, 35 mmol) was added, and the mixture was heated and stirred at the same temperature for 1.5 hours. The reaction mixture was diluted with water, 2M hydrochloric acid (0.5 mL, 1 mmol) was added, and the mixture was extracted with ethyl acetate (15 mL) two times. The organic layer was washed with 5% sodium bicarbonate aqueous solution (10 mL) and water (20 mL), and then dried with anhydrous sodium sulfate. The solvents were removed by distillation under reduced pressure, the residue was refined with silica gel column chromatography (Highflash 3L, manufactured by Yamazen Corporation, the mixture of hexane and ethyl acetate of 3:1 in mixing ratio), and colorless oily (1-nitro-cyclohexyl)-methanol (6.96 g) was obtained.

1. temperaturethe mixture was heated
2. additionwas added
3. extractionthe mixture was extracted with ethyl acetate (15 mL) two times
4. washThe organic layer was washed with 5% sodium bicarbonate aqueous solution (10 mL) and water (20 mL)
5. dry with materialdried with anhydrous sodium sulfate
6. customThe solvents were removed by distillation under reduced pressure
7. additionthe mixture of hexane and ethyl acetate of 3:1
8. additionin mixing ratio), and colorless oily (1-nitro-cyclohexyl)-methanol (6.96 g)
9. customwas obtained

ORD-Eintrag

ord-74b7df4c55644a818119d13f6e7b8b2a

Quelldatensatz

uspto-grants-2013_02

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08367666B2